Dr. Valentina MIHALACHE

Exchange biasing of oxide-DMSs (dilute magnetic semiconductors) in exchange bias nanostructures, which are essential for use in spin-based electronic devices, presents a challenge because, in the available literature, exchange coupling typically occurs between secondary phases, with oxide-DMS not being involved. The experimental results presented in this study are consistent with the participation of Fe-doped ZnO (oxide-DMS) as a ferromagnetic (FM) component in the exchange bias (EB) of the ZnFeO system. The study was conducted on ZnFeO nanostructured systems with a 2 at% iron concentration, which were processed by the decomposition of Zn-Fe-propionates and annealing in an Ar-5%H-2 atmosphere at temperatures between 480 degrees C and 510 degrees C and times between 60 min and 100 min. The magnetization investigations support the coexistence of an FM phase with a Curie temperature above 300 K, an antiferromagnetic phase with a Neel transition, T-N, at about 200 K and a disordered spin-glass-like phase with a transition, T-SG, at about 50 K. All samples show the EB effect, characterised by a high EB blocking temperature, T-B approximate to 200 K, and/or a low EB blocking temperature, T-B approximate to 50 K. The analysis of experimental data provides evidence for the exchange biasing of Fe-ZnO (oxide-DMS) by the FeO (AFM) phase and/or SG phase. The exchange-biasing of Fe-ZnO oxide-DMS is promising for developing new materials (e.g., FM electrodes) to improve the efficiency of injecting highly spin-polarised currents in spintronic devices and to increase the device operating temperature.

Preparation under non-identical conditions involving the reduction of sol-gel-derived precursors of various Zn:Fe atomic ratios (0.97:0.03, 0.8:0.2 and 0.4:0.6) in a hydrogen-containing atmosphere was used to obtain composites of nanosized ferromagnetic (FM) alpha-Fe and antiferromagnetic (AFM) FeO in different concentrations and of the desired magnetic responses. ZnO nanoparticles, developed in all preparation stages, served primarily as a matrix for the separation of Fe (and FeO) nanoparticles, preventing their agglomeration and coarsening. The average crystallite/particle size is about 5-32 nm, 10-75 nm and 21-31 nm for FeO, Fe and ZnO, respectively. Magnetisation investigations of FeO-Fe-ZnO nanocomposites revealed a coexistence of ferromagnetic and superparamagnetic behaviours ascribed to the Fe nanoparticles in different magnetic states. All samples exhibit the exchange bias effect, EB. Values up to 375 Oe for coercivity at 300 K, 600 Oe for coercivity, 223 for coercivity enhancement and 243 Oe for EB field at 5 K were measured. The magnitude of EB depends on the processing conditions - the EB field and coercivity enhancement are larger for samples processed under conditions of a higher degree of non-equilibrium. The presence of FeO appears crucial for the occurrence of EB, irrespective of its quantity. The EB is ascribed primarily to the exchange coupling between the AFM and FM spins at the FeO/Fe interfaces of nanostructures after field-cooling from above the TN of FeO and below the Curie temperature of Fe. An approach based on magnetically disordered AFM/FM interfaces featuring like spin-glass systems was adopted to explain the EB effects. An aspect of practical relevance is the suppression of room temperature coercivity in apparent correlation with the training of the EB; an attempt has been made to understand the origin of this suppression.

Zn1-xFexO nanoparticles with the iron concentrations level in the dilute regime (x = 0.001---0.01) were produced by a sol-gel route from acetate precursors along with an un-doped and 3 at.% Fe-doped reference. The X-ray diffraction of the un-doped and 0.1-1 at.% Fe-doped samples reveal the reflections for only the ZnO wurtzite structure. Fe doping enhances the a-axis lattice constant, the unit cell volume and the microstrain. Iron doping reduces the average crystallite/particle size (confirmed by Scanning Electron Microscopy), improving the surface-to-volume ratio or the concentration of defective surface sites. XPS identifies the iron in both Fe3+ and Fe2+ states. XPS and Fe-57 Mossbauer spectroscopy indicate a broad distribution (distortion) of Fe3+ sites on the surface of ZnO nanoparticles. The blue shift and broadening of the UV emission, and quenching of defect-related photoluminescence in the Fe-doped samples verify the presence of iron in the ZnO lattice and surface intrinsic defects. 0.1-1 at.% Fe-doped ZnO show room temperature ferromagnetism, RTFM, characteristic of dilute magnetic semiconductors, DMS. The magnetization measurements with temperature evidence an antiferromagnetic alignment and an increase of ferromagnetic contribution with Fe doping up to 1 at.%. Zn0.97Fe0.3O reference is a superparamagnetic ZnO/ZnFe2O4 nanocomposite with a blocking temperature of 20 K; HRTEM shows (ultra)fine ZnFe2O4 particles at the surface of ZnO nanoparticles. The analysis of experimental data of 0.1-1 at.% Fe-doped ZnO was done in terms of iron coupling with intrinsic defects, which can generate surface Fe3+ states with geometries similar to the Fe3+ in inverse spinel ZnFe2O4. The superexchange interaction (resembling that in the inverse spinel ZnFe2O4) between the Fe3+ sites with distorted configuration resulting in ferrimagnetism was hypothesised as a possible mechanism of RTFM. Experimental (structural, local chemical, magnetic, optical) and interpretation results can be used to optimize the processing conditions for Fe-doped ZnO to serve as an effective DMS, e.g. for spintronic applications.

We report in this paper on the monolayer composites thin films that have the magnetic spinel CoFe2O4 and the piezoelectric perovskite BNT-BT0.08 as constituent phases. Composite thin films of CoFe2O4 and BNT-BT0.08, with molar ratios of 0.5:1, 1:1 and 1.5:1, have been deposited by spin coating method from a sol precursor, mixture type, of CoFe2O4 and BNT-BT0.08. The monolayer thin films, deposited on Si/SiO2/TiO2/Pt substrate, were characterized using selected methods, such as: X-ray diffraction, scanning electron microscopy, atomic force microscopy/piezoelectric force microscopy, dielectric spectroscopy, and vibrating sample magnetometer. X-ray diffraction demonstrated the two phases: cubic CoFe2O4 and rhombohedral BNT-BT0.08. Furthermore, the Si/ SiO2/TiO2/Pt/BNT-BT0.08/CoFe2O4 monolayers show a simultaneous enhancement of both the magnetization and coercivity with the increase of the magnetic phase, accompanied by a decrease of the dielectric constant. The obtained results reveal that the investigated monolayer structures present superior properties compared to those of bilayer composites.

Nano-nitride reinforcement of Fe-Cr alloys are under intense investigations, e.g., along with oxide-strengthened, nitride-strengthened reduced activation steels with superior high temperature mechanical properties are developed as materials for nuclear energy applications. Fe14Cr alloy powders were produced by mechanical milling for up to 170 h under a nitrogen atmosphere followed by heating under an Ar5%H-2 atmosphere to 600 degrees C-1120 degrees C. The samples were investigated by means of X-ray diffraction, DTA/TG and magnetic measurements. CrN, detected after milling for 58 h, reached 39 wt % (5.3 wt.% total N) at 170 h milling. The ferrite supersaturated with nitrogen shows a strong decrease in grain size and saturation magnetization, an increase in lattice constant, microstrain and coercivity, H-c. Upon heating, the metastable ultrafine alpha-ferrite and CrN in the as-milled samples undergo transformations and recrystallization into ferrite grains free of super-saturation, whose microstructure follows a continuous relaxation. The supersaturation with nitrogen was retained upon heating in the relatively stable ferrite crystalized at the milling stage. This microstructure undergoes a discontinuous relaxation in the 800 degrees C-1120 degrees C region: a pronounced decrease of grain size (down to similar to 25 nm), an increase of lattice constant, microstrain and H-c. These improvements were associated with features of discontinuous precipitation reaction of coherent nitride precipitates (involving a new alpha ''-phase with expanded lattice), in connection with the heating in the austenite phase field. Such microstructure refinement or (nitride) strengthening of Fe14Cr alloys can be achieved on powders milled for much less time as compared to previously reported (oxide dispersion) strengthening of Fe14Cr-W-Ti ferritic steels. (C) 2022 The Authors. Published by Elsevier B.V.

Zn-Fe-O nanoparticle systems (Z3F, Z20F and Z60F) were produced by changing the Zn:Fe ratio (0.97 : 0.03, 0.8 : 0.2 and 0.4 : 0.6 in at%, respectively) in Zn(ii)-Fe(iii)-carboxylate precursors. According to X-ray diffraction, Z60F is nearly single-phase ZnFe2O4 (5.9 nm crystallite size), Z20F is a ZnO/ZnFe2O4 nanocomposite consisting of 48.8% ZnFe2O4 (4.7 nm crystallite size), and Z3F is apparently pure ZnO (9.5 nm). We found evidence for a ZnFe2O4 spinel of high inversion degree (80-100%) and with superparamagnetic (SPM) behaviour at room temperature in all three samples by a remarkable correlation between HRTEM, FTIR, XPS, Mossbauer and magnetization analyses. Iron modifies the decomposition process of the precursor and enhances its viscosity, which appears to favour the separation of Zn- and Fe-rich phases. As a consequence, two-phase systems of individual nanocrystals/nanoparticles (ZnO and ZnFe2O4) are formed. The large anisotropy constant, 10(6)-10(7) erg cm(-3), of the ZnFe2O4 nanoparticles and the concentration dependence of their magnetic energy barrier are explained in terms of interparticle interactions interlinked with finite size effects and high inversion degree; these factors also control the other parameters of importance for applications, including the blocking temperature (13-111 K), saturation magnetization (1.08-17.7 emu g(-1) at 300 K, 4.6-44.8 emu g(-1) at 5 K) and coercivity (85.4-491 Oe at 5 K). Magnetic dynamic results, particularly modelled by the Neel-Brown and Vogel-Fulcher laws, yield fitting parameters which validate the presence of concentration-dependent dipole-like interactions between ZnFe2O4 nanoparticles. A fraction of iron was found in the Fe2+ state, presumably substituting for Zn2+ in zinc oxide; however, the samples behave like ZnFe2O4 SPM nanoclusters/nanoparticles dispersed in a nonmagnetic ZnO particle assembly, rather than Zn(Fe)O dilute magnetic semiconductors. The relevance of the properties of the investigated material for specific applications is highlighted throughout the manuscript.

ZnO nanostructures with intrinsic and extended defects were prepared by rapid decomposition of zinc-propio-nate and annealing at 400 degrees C-970 degrees C. The correlation between the structure/morphology, type of native defects (photoluminescence (PL), EPR) and ferromagnetism was investigated, together with ammonia adsorption capacity. All the samples show room temperature ferromagnetism (RTFM). Crystallite size increases while the unit cell volume, c-axis constant, microstrain and saturation magnetization relax with increasing temperature; morphology varies from aggregated nanoparticles to frameworks of well-welded crystals. 400 degrees C-800 degrees C annealed samples show a broad visible and/or a prominent violet-blue PL emission and, two narrow g = 2.0065 and g = 1.9632 EPR signals. 800 degrees C-970 degrees C annealed samples exhibit very intense green-yellow photoluminescence. The intrinsic defects in conjunction with a deformed lattice and/or pinned by grain-boundaries appear responsible for RTFM and Curie temperature exceeding 700 degrees C. Tuning the morphology, PL intensity and ferromagnetic signal by choice of annealing temperature can find applications in (gas) sensing, photonic/optoelectronic and spintronic devices.

Oxide dispersion-strengthened ferritic steels (ODSFSs) are promising structural materials for applications in fusion and fission power reactors, but further improvement in their (high-temperature) mechanical properties and ferrite phase stability is required. This work demonstrates that an approach to produce Fe14Cr ODSFSs with a stable ferrite phase and improved strength could involve grain size strengthening by long-term milling with a tiny amount of nitrogen. Fe-14Cr-3W-0.4Ti-0.25Y(2)O(3) powders were ball-milled up to 170 hours under an argon atmosphere. In addition to X-ray diffraction, the change in product quality during milling and upon heating was thoroughly investigated by more sensitive magnetic and thermal analysis by measuring the saturation magnetization sigma(s), coercivity H-c, Curie temperature T-c, and temperature of ferrite-austenite (alpha ->gamma) transition T-alpha ->gamma. A pronounced modification of magnetic and microstructure parameters was observed when milling over 70 hours and upon heating above 800 degrees C and was found to be generated by long-term milling with a tiny amount of nitrogen. Upon heating, the nitrogen, incorporated during milling, developed a transition region, with the decomposition of nitrides precipitated at the earlier stage of heating followed by austenite decomposition, nitrogen degassing, and microstructure refinement to a grain size of a few tenths of a nm (e.g., 28 nm by heating at 910 degrees C of 100-hour milled powder). The resulting ferrite phase with refined grains is highly stable to (further) heating. The powders milled for 70 and 100 hours containing 0.175 and 0.500 wt pct nitrogen, respectively, were consolidated at 1100 degrees C with subsequent annealing at 1050 degrees C and subjected to Vickers hardness and 3-point bending tests. The steel produced from the powder milled for 70 hours shows lower hardness, higher density (close to the theoretical value of 7.8 g/cm(3)), and fracture strain. The ductility of this ODS alloy (0.075 fracture strain) is comparable with Eurofer97 (0.075 fracture strain), whereas its strength (2070 MPa ultimate stress) is significantly higher than that of Eurofer97 (1222 MPa ultimate stress). This improvement was attributed to grain size strengthening-the refined grains (promoted by milling with nitrogen) could be effectively pinned by Y-Ti-O dispersoids.

Fe-14Cr-0.4Ti-0.25Y(2)O(3) ferritic steels were produced by varying the amount of residual process control agent, PCA (ethanol), in the ball-milled powders and changing the spark-plasma-sintering, SPS, temperature. Near the-oretical density (99.3%), high Vickers hardness (501-920 HV, measured by applying a load of 100 g for 5 s) and fine grain size (26-36 nm), very stable against heating, can be achieved on ODS ferritic steels, consolidated from powders with a low amount of PCA and processing temperature in the range of 1000 degrees C-1100 degrees C. Additional grain refinement occurs near alpha -> gamma transition which is generated by the reaction of the traces of PCA with the ferritic matrix upon heating. High local temperatures and the evolved thermally activated processes, at the contact points between particles/at the particle surfaces during SPS-consolidation, were demonstrated to be the main factors responsible for improved densities and hardness. The role of PCA in the sintering, thermal and microstructure particularities and its impact on the quality of the final steel was thoroughly analysed throughout the work. (C) 2019 Elsevier B.V. All rights reserved.

We report on the influence of dilute doping combined with the processing conditions on the morphological, structural, chemical states, photoluminescence and magnetic properties of Zn1-xNixO nanopowders. Ni doping changes the ZnO powder morphology from randomly-aggregated nanocrystals to densely-packed nanocrystals arranged in columnar particles, modifies the high-energy-component of O1 s spectrum and increases the modified Auger parameter in XPS, enhances the blue photoluminescence (PL) emission, suppresses the green PL emission and the intensity of the g = 1.997 EPR signal. Ni-ZnO nanostructures show room-temperature ferro-magnetism (implying they can serve as dilute magnetic semiconductors). The saturation magnetization, crystallite size and microstrain increase with the doping level; the c-axis constant and unit cell volume decrease, however, being unexpectedly higher with respect to a (reference) ZnO powder with a relaxed lattice. We demonstrate that the investigated properties were controlled by both (dilute) doping level and donor native defects produced by non-equilibrium (oxygen-deficiency and high rate of) ZnO formation.

Four batches of cerium oxide powders (with nanocrystallite size of 6.9 nm-572 nm) were prepared from four precursor nanopowders by thermal decomposition of Ce-propionate and annealing in air between 250 degrees C-1200 degrees C for 10 min-240 min. Ceria formation reactions, structure, vibrational, luminescence and magnetic properties were investigated by differential scanning calorimetry, x-ray diffraction, electron microscopy, infrared spectroscopy, photoluminescence and SQUID. All the samples exhibit room temperature ferromagnetism, RTFM, (with coercivity, H-c, of 8 Oe - 121 Oe and saturation magnetization, M-s, of up to 6.7*10(-3) emu/g) and a broad defect-related photoluminescence, PL, emission in the visible range. The samples derived from the same precursor show M-s proportional to the peak area of defect-related PL emission whereas this is not valid for the samples derived from the different precursors. An improvement of ferromagnetism and intensity of defect-related PL emission was observed when annealing the products in which nanocrystalline cerium oxide coexists with Ce - oxicarbonate traces, Ce2O2CO3. The experimental results were explained based on the following considerations: room temperature ferromagnetism was induced by the defective ceria with high concentration of oxygen vacancies generated by decomposition of Ce-propionate; oxygen vacancies of the starting precursor nanopowders could be redistributed (at the surfaces/grain boundaries, GBs) upon heating under conditions that promote an inert local environment; the decomposition of Ce2O2CO3 residues can provide an excess of oxygen vacancies at the nanoparticles surfaces or GBs, which can induce or enhance ferromagnetism; surfaces/GBs rather than bulk defects appear responsible for RTFM - this can explain the (often reported in literature) inconsistency between oxygen vacancies concentration and M-s. (C) 2018 Elsevier B.V. All rights reserved.

Refined structure of the ferritic phase induced by mechanical milling (under reducing atmosphere) and its thermal stability are required in various applications of nanostructured ferritic alloys. The impurification with nitrogen and oxygen uptaken from the air is very probable during ball-milling, especially at the long-time high-energy milling conditions. As a rule, these interstitial impurities in as-milled powders are in quantities under the sensibility limit of conventional measurement techniques, such as XRD and SEM/ EDS. To evidence the tendency for microstructure modification by impurities introduced during milling, the Fe-14Cr-3W-0.4Ti-0.25Y(2)O(3) (Fe14Cr) ferritic steel powders (re)loaded in air and milled up to 170 h with interruption of the milling process, and heated up to 1373 K were investigated by thermal analysis in correlation with X-ray diffraction and scanning electron microscopy. XRD failed to detect the impurities in powders milled up to 38 h in air although a consistent mass loss related to the degassing of N-2 was registered in thermogravimetric, TG, curves. (Fe,Cr)(4)N, fcc-c, (Fe, Cr)(2)O-3 impurity phases in powders milled over 38 h in air and (Fe,Cr)(2)O-4 formed upon heating were readily detected by XRD. The analysis of these results allowed to better understand the impurification process and to generalise it for any as-milled Fe-Cr-based alloy powder processed in any milling conditions irrespective of the milling atmosphere, duration and thus, of amounts of contaminants. The quality of three powders milled for 170 h in three different conditions was compared: in air, under an argon atmosphere with interruptions of the milling process and under an argon atmosphere without interruption of the milling process. The contamination of powder milled for 170 h under an argon atmosphere without interruption of the milling process is insignificant (corresponding to less than 0.5 mass% mass loss in TG) as compared to powders obtained in the other two milling conditions. New approaches for minimising the contamination from air are suggested.

Fe doped ZnO particles of flower-like shape, hexagonal prisms and hybrid structures flower-prisms have been synthesized by hydrothermal technique, and their luminescence and magnetic properties have been investigated as a function of the morphology changes due to iron dopant (0-0.03 at.% Fe3+). The X-ray diffractograms of Zn1-xFexO powders indicated a hexagonal wurtzite polycrystalline structure. SEM images reveal the change of Zn1-xFexO grains shape from flower-like to hexagonal prisms as the Fe concentration (x) increases from 0 to 3 at.% Fe. Undoped ZnO shown weak room temperatures ferromagnetism, with high coercivity (H-c = 107 Oe) and saturation magnetization M-s of 1.5-10(-3) emu/g. ZnO doped with 1 and 3 at.% Fe presented a significant increase of the magnetization in comparison with the undoped ZnO. For ZnO doped with 3 at.% Fe, Ms = 32.5-10(-3) emu/g and M-rem = 0.78-10(-3) emu/g. Compared with other reports on magnetic properties of undoped and Fe doped ZnO, these results indicated higher coercivity and smaller magnetizations. The drop in the intensity of characteristic green-yellow photoluminescence band of ZnO at about 550-600 nm was attributed to the decrease of the number of oxygen vacancies and interstitial oxygen. By increasing the Fe concentration, the electron paramagnetic resonance (EPR) signal of undoped ZnO decreases due to the decrease of defects concentration. (C) 2017 Elsevier Ltd. All rights reserved.

Cobalt ferrite (CF) powder was synthesized by solid state reaction method at two different calcination temperatures (1120 K and 1320 K) then milled in two steps, gradually reducing the milling media size. The first milling step results in CF nanoparticles with crystallite size of 33 nm showing fairly high coercivity (3.7 kOe), > 5 times higher than the non-milled material (0.7 kOe). The high coercivity was correlated to the crystallite size close to the single-domain limit, and to the strain increase up to 2.1%. This value of strain is the highest ever reported in literature for the CF and brings to the highest figure of merit for permanent magnets, (BH)(max)= 2.16 MGOe. After the second milling step the powder displays particle size of 9 nm, release of strain (epsilon = 1.2%), coercivity reduction that approaches 250 Oe and decrease of the deblocking temperature from 421 K to 317 K. The large tunability obtained by multi-step milling allows to use CF in different applications. In particular, the milled CF powder characterized by high microstrain is a good candidate for the realization of rare-earth-free permanent magnets (at least on the basis of the (BH)(max) product). For the first time, a correlation between the spin-canting angle and the degree of inversion, the crystallite size and the microstrain is presented and discussed. [GRAPHICS] .

The magnetic properties, in the 5 K-350 K temperature range, were investigated in relationship with the structure and morphology of Zn1-xFexO (x = 0, 0.01, 0.03) powders prepared by hydrothermal route. The magnetization measurements reveal that all powders are ferromagnetic at room temperature, with Curie temperature TT, higher than 350 K. The coercivity Hc takes values between 58 Oe and 107 Oe at 300 K and, between 217 Oe and 613 Oe at 5 K. The weak magnetization of the un-doped ZnO powder is temperature independent and was associated with the high surface to volume ratio of the powder particles (or the number of surface defects). The saturation magnetization M-s, was substantially enhanced (up to a factor of about 20 at 300 K and of about 200 at 5 K) at all temperatures as Fe concentration increased, in spite of reduction of the surface to volume ratio of the powder particles. The Hc vs. Tand FC/ZFC curves for the un-doped ZnO show typical ferromagnetic behavior, whereas for the Fe doped powders exhibit Ruderman-Kittel-Kasuya-Yosida (RKKY) - like and spin-glass-like behavior. The observed magnetic phenomena in Fe doped ZnO can be explained on the basis of "donor defects concentration magnetic cations concentration" phase diagram for dilute magnetic semiconductors. (C) 2017 Elsevier B.V. All rights reserved.

Commercial MgB2 powder was loaded into a Fe-tube, by plastic deformation a tape of similar to 0.5 mm in thickness and 6.9 mm in width was obtained. Short pieces were processed by Spark Plasma Sintering (SPS) at 950, 1050 and 1150 degrees C for 3 min. The optimum sintering temperature is 1050 degrees C. From magnetic/electrical measurements, the onset critical temperature and the irreversibility field at 5 K were 38.7 / 38.9 K and 6.2 / 13.5 T, respectively. The pinning-force-related parameters indicate that the dominant flux pinning mechanism is of point pinning type. Contribution of grain boundary pinning is stronger at lower temperatures.

Cobalt ferrite (CoFe2O4) has been successfully synthesized by sol-gel technique. Pellets were prepared by spark plasma sintering technique (SPS) from CoFe2O4 sol-gel derived powder. The rapid sintering of CoFe2O4 pellet by SPS at 950 degrees C, leads to a dense ceramic (97%(rho theoretic)) with average crystallite size of 71 nm. As revealed by X-ray diffraction and Mossbauer measurements, the obtained powder and SPS pellets are spinel ferrite with a cubic symmetry. Complex dielectric investigation performed on CoFe2O4 ceramic reveals multiple relaxation mechanisms while the magnetic measurements indicated a saturation magnetization value of similar to 83 A m(2)/kg at room temperature, which make them useful for applications in microwave domain. (C) 2015 Elsevier B.V. All rights reserved.

The contamination from the air (the identification of the impurity phases and their thermal evolution) of Fe-14Cr-3W-0.4Ti-0.25Y(2)O(3) oxide dispersion-strengthened ferritic steel powders ball-milled for different times was evidenced by thermal analysis in correlation with X-ray diffraction and scanning electron microscopy. The powders loaded under an argon atmosphere and milled up to 170 h with and without interruption of the milling process were compared. A steady state of Fe-Cr alloying was reached within the first 12 h. The reflections corresponding to a new phase with an fcc-CrN structure were found in XRD patterns of powders milled for a long time with interruption. The differential thermal analysis of powders milled over 12 h with interruption shows an exothermic peak at 625.5-653 degrees C, ascribed to the coarsening of the fcc-CrN, and an endothermic reaction above 1000 degrees C accompanied by a mass loss in thermogravimetric analysis. (Cr,Fe)(2)O-3 and retained austenite were also found upon the heating of as-milled (with interruption) powders to different temperatures. The endothermic feature was associated with the decomposition of CrN accompanied by the degassing of N-2. The observed phenomenon was explained to be the manifestation of contamination with nitrogen and oxygen from the air during the milling; the rate of contamination with nitrogen was estimated to be 0.011 mass% h(-1). The contamination level depends on the degree of alloying at the moment of the interruption of milling process. The contamination of the powders milled without interruption of milling process was insignificant. The experimental conditions described in this work can be further developed for the removal of impurities (e.g. nitrogen, nitrides, oxides) from alloyed ferritic steel powders.

Powder mixtures of MgB2 and B4C with composition ((MgB2) + (B4C) x, x = 0.005, 0.01, 0.03) were consolidated by Spark Plasma Sintering at 1150 degrees C for 3 min. The average particle size of B4C raw powder was relatively high of 4 mm. Despite this, it is shown that processing processes are fast and, as in the case of the in-situ routes, for our ex-situ method carbon substitutes for the boron in the crystal lattice of MgB2. Specifics of microstructure are discussed based on electron microscopy observations. Carbon substitution and microstructure contribute to enhancement of the critical current density J(c) at high magnetic fields and of the irreversibility field H-irr. Samples are shown to be in the point pinning limit with some tendency toward the grain boundary pinning depending on B4C doping amount and temperature. An optimum composition is found for x = 0.01: for this sample, at 20 K, a J(c) of 100 A/cm(2) is obtained at 5.35 T. This value is higher than for the pristine MgB2 sample and for an optimum ex-situ nano-SiC-doped sample obtained for the same SPS processing conditions. (C) 2015 Elsevier B.V. All rights reserved.

Dense samples (relative density > 93%) of bulk MgB2 with GeO2 additions were obtained by Spark Plasma Sintering. The critical current density J(c) of the added samples is improved at high magnetic fields when compared to the pristine sample. The optimum composition is for MgB2(GeO2)(0.005). For this sample, a J(c)(20 K) = 10(2) A/cm(2) is obtained at 5.1 T versus 3.9 T for the pristine sample. Ge substitution in the crystal lattice of MgB2 can be considered negligible, and T-c,T-onset and T-c,T-midpoint from magnetization measurements scatter within 0.2 and 0.6 K, respectively. TEM investigations show some specific details at nano scale: the tendency to form secondary phases (25-100 nm) with sphere-like or irregular shapes is observed and discussed. Samples are composites and the residual strain of MgB2 is constant for pristine and GeO2-added samples. Therefore, pinning enhancement leading to improvement of Jc for the GeO2 added samples is purely a 'microstructure' effect due to the presence of secondary phases. The point pinning is determined to be the predominant mechanism. Addition of a higher amount of GeO2 is shifting the pinning mechanism toward a grain boundary pinning. (C) 2015 Elsevier Masson SAS. All rights reserved.

YBa2Cu3O7-delta films were deposited on CeO2-buffered nickel substrates, with different buffer thickness. Full width at half maximum of rocking curve, Delta(omega), of CeO2 and yttrium barium copper oxide (YBCO), as well as the critical temperature, T-c, of YBCO were shown to be strongly dependent on buffer thickness. They behave similarly but not proportional to the buffer thickness increase. This and the fact that Delta(omega) vs. buffer thickness and T-c vs. buffer thickness for YBCO behave similar with RMS roughness vs. thickness of CeO2 indicates that the surface peculiarity of buffers is responsible for YBCO properties. More precisely, the surface of CeO2 films prepared by the chemical solution route based on propionic acid is prone to agglomerate (de-wet) and the degree of agglomeration depends in an intricate way on buffer thickness. We showed that nor RMS roughness neither (00l) texture degree can define alone the surface suitable for c-axis YBCO nucleation. The {111} faceted grains (even in the case of high (00l) texture) and other defects generated by agglomeration supply a low fraction of (00l) flat terminations of buffer that affect the nucleation of c-axis-oriented YBCO phase. Moreover, the thermal instability of the surface morphology of CeO2 buffers (further development of de-wetting process, {111} faceted grains, etc. during superconducting layer deposition) influence the quality of YBCO films.

ac susceptibility measurements as a function of temperature T and the ac magnetic field amplitude, Hac, have been performed on five superconducting Bi1.8Pb0.4Sr2Ca2-xYxCu3Ox polycrystalline samples (x = 0, 0.005, 0.04, 0.15 and 0.36, and with the volume fraction of the Bi2Sr2Ca2Cu3Oy (2223) phase, f approximate to 100%, 100%, 64%, 0% and 0%, respectively. By using the Muller model for granular superconductors, we found that the pinning force density obtained from the imaginary peak of chi ''(T) is strongly dependent on the doping level. To describe this dependence we adopted the multilayer model (a stack of superconducting, S, and normal, N, layers) of a superconductor. In the framework of this model, we demonstrated that (a) the yttrium addition influences the degree of coupling between the adjacent S layers (and thereby, the pinning strength) through the modification of the carrier concentration and of the effective thickness of the N layers, and (b) the intergrowth of Bi2Sr2CaCu2O delta (2212) layers within the 2223 grains has an important influence on the thickness of N. (C) 2011 Elsevier B.V. All rights reserved.

CeO2 films were prepared from solutions of different concentrations (0.05-1.0 M) on textured Ni substrates. Homogeneous nucleation and growth of CeO2 nanocrystals 170 nm (>0.8 M), the transition to classical curvature-driven grain-growth kinetics is evident (at 1000 degrees C, below the literature value of 1100 degrees C). The decrease in the Kohlrausch exponent for these thick films suggests that the grain coarsening through grain boundary migration is responsible for the stretched regime of grain-size relaxation. (C) 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Barium titanate (BaTiO3) has been doped in situ with 5 mol% thulium by a sol-gel method. The as-prepared gel powder consists of nanosized grains (20-30 nm) and crystallizes on the cubic BaTiO3 lattice, at 700 degrees C. Ba0.95Tm0.05TiO3 ceramics derived from this powder have tetragonal perovskite structure and contain a small amount of Tm2Ti2O7 pyrochlore phase. These ceramics exhibit dielectric constants of 4282-3240 and dielectric loss (tan delta) of 0.1077-0.0161 at Curie temperature T-c=132 degrees C and at 10 Hz-100 kHz, respectively. For a drive voltage of 400 V, the hysteresis loop recorded at the frequency of 100 Hz shows a remnant polarization (P-r) value of 76 mu C/cm2 and a coercive field (E-c) of 124 V and for 1 kHz a remnant polarization (P-r) value of 58 mu C/cm2 and a coercive field (E-c) of 116 V.

The first field for magnetic flux penetration H in Bi2Sr2CaCu2O8+delta (Bi-2212) single crystals near the critical temperature T-c was investigated from the local magnetic hysteresis loops registered for different magnetic field H sweeping rates by using a scanning Hall probe microscope (SHPM) with similar to 1 mu m effective spatial resolution. Evidences for a significant role of the surface barrier were obtained: the asymmetric shape of the magnetization loops and an anomalous change in the slope of H-p(T) close to T-c. (C) 2011 Elsevier B.V. All rights reserved.

Scanning Hall probe microscopy with an effective spatial resolution of similar to 1 mu m has been used to investigate the vortex structures in superconducting Bi2Sr2CaCu2O8+delta single crystals in the temperature range 77.3-81.3 K and zero applied field (in the presence of the earth field). The vortex images were obtained in real time mode as the temperature increased slowly for 3.36 h. At 77.3 K, the vortices were arranged in a chain structure. With the increase of the temperature, two jumps in the vortex array occur at 77.3 K, immediately when the temperature starts to rise, and at 79.2 K with a good stability between jumps. The second jump is accompanied by the jump in the average magnetic induction when bundles of 4-5 additional vortices enter the scanning area and the vortex array get disordered. These directly visualized transitions in the vortex lattice are consistent with a vortex creep over the surface barriers at high temperatures. A short movie is presented. (c) 2008 Elsevier B.V. All rights reserved.

ac susceptibility measurements were performed on pure and SiC-doped MgB2 prepared by field assisted sintering technique in the temperature range between 5 and 50 K. The activation energy for flux-creep U for both samples was determined at dc-fields of 0, 0.5, and 5 T, respectively, from the frequency dependence of the imaginary part of the ac-susceptibility chi '' data measured in the range 17-9997 Hz. It was found that at 0 and 0.5 T, the activation energy of the SiC-doped sample is almost half the energy of the pristine sample whereas at 5 T the activation energies of the two samples become almost equal. A similar behaviour show the H-p(T) lines as obtained from susceptibility data in the range 0-9 T. For fields lower than 7.5 T, the H-p field of the doped sample is lower than for the undoped MgB2. At similar to 7.5 T, the H-p(T) for SiC doped MgB2 crosses over the H-p(T) of pure MgB2 and for higher fields the doped samples exhibits a higher irreversibility H-p. This field dependence was extracted from the evolution of the. chi(1)''(T) data. This behaviour is a consequence of the morphology of the sample with a large spread in grain size.

Fundamental and third harmonic ac susceptibility measurements as a function of temperature T, ac magnetic field, and dc magnetic field have been performed on Bi(Pb)SrCaCuO/2223 bulk samples consisting of both Bi2Sr2Ca2Cu3O10+delta (2223) and Bi2Sr2CaCu2O8+delta (2212) phases. Since the chi(1)''(T) peak corresponding to the losses in the weak links between the grains shifts rapidly to lower T and its amplitude is strongly suppressed with increasing the dc magnetic field H-dc, the other peaks related to the losses in the grains become visible. For the samples consisting of single phase 2223, these intragranular peaks are situated near 38 K, 58 K, and 80-88 K (depending on the sample), whereas for the samples consisting of single phase 2212, they are situated near 20 K, 43 K, and 77 K. For H-dc >= 1 kOe, the temperature positions of the intragranular peaks are weakly field dependent. This shows that the transition line determined from the loss peaks behaves like the melting line in two-dimensional (213) systems. Also, as the field increases, the amplitude of the loss peaks can decrease up to their disappearance, suggesting a layer decoupling process. In this way, we show that, above a crossover field of similar to 1 kOe, the vortex lattice in the superconducting grains of polycrystalline samples reproduces the behaviour of the vortex lattice in a quasi-2D object consisting of a set of separated "thin films" with one-, two-, and three-effective-layer thicknesses. For the samples consisting of both 2223 and 2212 phases, three additional peaks were observed, situated near 28 K, 50 K and 75-80 K (depending on the sample). These peaks were attributed to the regions in which the 2212 and 2223 layers alternate. (c) 2007 Elsevier B.V. All rights reserved.

High harmonics ac susceptibility measurements joint with neutron irradiations on quasi-bi-dimensional high temperature superconductor (quasi-2D-HTSC) are good tools to study the flux dynamics and its interaction with pinning processes in these superconductors. Flux neutron intensity of 5 * 10(17) n * cm(-2) shows a deep change in the flux pinning dynamics in Bi-Sr-Ca-Cu-O (BSCCO) system. Third harmonic susceptibility signal increases in amplitude after the neutron irradiation, followed by a rise of the pinning and critical current. Moreover, after the irradiation, the measurements underline the demise of the anomalous peak effect (PE) associated with a three-dime.nsional/two-dimensionaI (3D/2D) flux lattice transition.

Samples of (Bi,Pb)(2)Sr2Ca2Cu3O10 (Bi(Pb)-2223) phase have been fabricated from two different oxide precursors with the same stoichiometry, synthesized by solid state reaction in the air at 815 degrees C for 20 h. The first precursor was prepared by mixing Bi2O3, PbO, SrCO3, CaCO3 and CuO powders, while the second one through mixing Bi2O3 and PbO with Sr2Ca2Cu3Ox produced from SrCO3, CaCO3 and CuO powders. Pellets from the two precursors were prepared in the same conditions; heat treatment time was varied and intermediate grindings were applied. Although the maximum attained Bi(Pb)2223 phase amount was about 50% and above 90% in the samples from the two precursors, respectively, the samples from the first precursor have generally shown better superconducting properties such as the critical temperature from resistivity measurements and intragrain critical current J(cg) from magnetic susceptibility measurements. For our particular case the influence of the final heat treatment is relatively low and at the same time the precursor plays a major role in controlling growth processes and final superconducting properties. Lower room-temperature Seebeck coefficient of the thermoelectric power for the samples fabricated from the first precursor suggests that one mechanism through which this control is realized might be the modification of the oxygenation level in the samples produced from different precursors. It was also found that for the samples prepared from the two precursors, intermediate grinding after 110h or more of heat treatment enhances density, almost does not influence J(cg) (or slightly improves it), decreases T-c, and does not influence significantly the amount of Bi(Pb)-2223 phase.

The critical temperature, T-c, for (Bi,Pb)Sr(Ca2-x, Y-x)CuO/2223, with x between 0 and 0.45, polycrystalline samples have been investigated. T-c of (Bi,Pb)(2)Sr2Ca2-xYxCu3O10+delta phase, 2223, found in samples with x 0.05, displays a parabolic dependence with the increase of Y content. The change of T-c for 2223 originates mainly from the increase of x. The variation of both x and oxygen content, delta, influences the T-c of 2212. The doping state of 2212 and 2223 in Y substituted samples suggests that, generally, in the samples consisting of both superconducting phases, 2212 is in over-doped state whereas 2223 is in under-doped state. The last affirmation suggests that 2212 could bring a significant contribution in the transport parameters of (Bi,Pb)SrCaCuO/2223 samples.

The superconducting properties of iodine-intercalated high-temperature superconducting Bi2Sr2Ca2Cu3O10+x phase (Bi-2223) were systematically studied. It was found that for samples containing a significant amount of Bi2Sr2CaCu2O8+x , iodine intercalation results in the dramatic decrease of the inter-granular critical current density, as well as a significant decrease of the critical temperature (T-c), the critical current density in the grains (J(cg)), and of the amount of Bi-2223. For samples with a large amount of Bi-2223, T-c changes insignificantly, whereas J(cg) can even increase. We argue that the different behavior of the superconducting parameters is the result of various oxygen concentrations, and we explain the effect of iodine intercalation based on the parabolic dependence between T-c and the number of holes per CuO2 layer. The H(T) curves (determined from the peak position in the loss signal of ac susceptibility) for intercalated samples deviate significantly from the quasi 2D-like behavior, pointing toward an enhancement of the 3D fluctuations of vortices. For the change in the values and dimensionality of the flux pinning in the process of the intercalation, we attempted a qualitative explanation based on the models proposed in literature.

We investigated the superconducting parameters of iodine-intercalated BiSrCaCuO high-temperature superconducting materials. While for samples containing a significant amount of Bi2Sr2CaCu2O8+x, (Bi-2212) iodine intercalation results in the dramatic decrease of the superconducting parameters, it was found that for samples with a nearly single Bi2Sr2Ca2Cu3O10-y (Bi-2223) phase these parameters can increase. We argue that this different behavior of the superconducting parameters is the result of a different doping regime, and can be explained based on the parabolic dependence between T, and the number of holes per CuO2 layer. Iodine intercalation appears to be an efficient way to bring the usually under-doped superconductor to its optimal T-c and flux pinning properties.

We have studied a portion of H-T phase diagram of the anisotropic Bi2223 bulk system using multi-harmonic ac susceptibility measurements (chi(n)). Based on the behavior of the third harmonic modulus,vertical bar chi(3)vertical bar, the irreversibility line (IL) was obtained from the onset of vertical bar chi(3)vertical bar, and an anomalous peak effect (PE) was observed. It has been shown that the anomalous peak is due to the crossover between a three-dimensional (3D) and a quasi-two dimensional (quasi-2D) peculiarity of vortex dynamics, the crossover magnetic field being H-CR approximate to 0.1T. The obtained portion of B-irr(T) is well described by the melting line of the flux lattice. The 3D flux fluctuation part (low field and high temperature) is described by the nearly parabolic temperature dependence B=B-o(Tc/T - 1)" with n = 1.58 (sample 1) and n = 1.48 (sample 2). The other region (high field and low temperature) is well described by the temperature dependence of the quasi-2D flux fluctuations, T-m(H) = T-m(2D)[1 + b/(In B/B-cr )(1/v)] corresponding to the weak interaction between pancake vortices from adjacent planes. The 2D limit temperature was determined as T-m(2D) = 36.7K (sample 1) and T-m(2D) = 27.3K (sample 2). (c) 2005 Elsevier B.V. All rights reserved.

A scanning Hall probe microscope (SHPM) with an effective spatial resolution of 1 similar to mu m has been used to study the local induction in high quality superconducting Bi2Sr2CaCu2O8+delta single crystals at high temperatures and low magnetic fields. We observed, for the first time to our knowledge, an anomalous splitting of the peak of first full penetration of magnetic field, We discuss the observed splitting, which is connected to the effects of surface and geometrical barriers on the vortex lattice.

Using the transport and magnetization measurements, the influence of neutron irradiation at a fluence of 5 x 10(17) n cm(-2) on (B0.65C0.35)Ba1.4Sr0.6Ca2Cu3Oz has been investigated. The neutron irradiation was found to decrease critical temperature and transport critical current density, increase the residual and normal state resistivity, and improve the intragranular critical current density with 1.6 x 10(5) A/cm(2) (at 77.3 K and in the applied field up to 160 kA m) and Delta M-irr/Delta M-nonirr ratio (up to factor of 3) at highest field used for investigation. The field dependence of this ratio, which is below the unity at very low field but higher than I at high fields, correlated with the shape of the hysteretic loops as well as with the change of the transport parameters after irradiation suggests the role of the irradiation-induced effects on the grain edges. We discuss these effects in the framework of the Bean-Livingstone surface barriers and geometrical barriers.

The effect of LiF content on the 2223 phase of the high temperature superconducting system Bi1.8Pb0.4Sr1.8Ba0.2Ca2Cu3Ox/(LiF)(y) (y = 0.02 to 0.15) was investigated by means of magnetically modulated microwave absorption (MAMMA). The experimental results confirmed a two fold increase of the superconducting phase content together with a slight rise (around 2 %) of the critical temperature for y=0.07. At the same time, for y between 0.05 and 0.12 the -Delta T-c(mw)/Delta B ratio was practically constant and equal to (18.5 +/- 1.5) KT-1, a typical value for 2223 superconducting phase.

AC susceptibility measurements have been performed on Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox (Bi-2223) samples doped with different Li-based compounds and prepared by the solid-state method. As-prepared samples and/or samples annealed in oxygen or argon, ground or unground, have been investigated in detail in order to understand the occurrence, nature and evolution of the anomalous peaks observed in chi " (T) curves versus the measuring parameters; we have detected up to four peaks instead of the usual two peaks observed in the non-doped samples. It was found that intrinsic physical-chemical properties, such as the melting temperature of the doping compound, are no less important for the final properties of the superconductor than their insertion properties into the crystal lattice of Bi-2223. Doping compounds with melting temperatures below or close to the phase formation temperature of the Bi-2223 phase can act as flux, changing the growth conditions. Intensification of some processes against others (e.g. decomposition-recovery of the BI-2223 phase, solubilization-precipitation of the secondary phases, changes in the properties of the liquid phase, etc) can lead to the formation of the Bi-2223 phase with different properties than for the non-doped superconductor. Generally, when using flux-type doping compounds, anomalous AC losses peaks are detected and the intra-granular critical current density is enhanced.

We have investigated the effect of Li2CO3 addition on the transport and magnetic properties of Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox, samples in connection with the structural changes observed by scanning electronic microscopy (SEM) and X-ray diffraction. In addition to the results reported in literature, we have extracted new information from the magnetic hysteresis loops and AC susceptibility measurements. One such information is the splitting of the AC loss peak corresponding to the dissipation inside the Bi-2223 grains. The results reported here have been compared with those obtained for Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiF)(y) and Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiCl)(y) specimens, and the effect of halogen is pointed out. (C) 2004 Elsevier B.V. All rights reserved.

We investigated the superconducting critical temperature, the intra- and intergranular critical current density, and the thermopower properties of Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiCl)(y) samples. All these properties have been compared with those of Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiF)(y) specimens. It was found that the critical temperature determined from resistive and AC complex susceptibility measurements show a maximum and the transition width shows a minimum for the intermediate values of y. Powder X-ray diffraction studies and the AC complex susceptibility measurements reveal that in our samples the amount of Bi2Sr2Ca2Cu3O10+delta high-temperature superconducting phase is maximum for y approximate to 0: 02: The amount of LiCl in Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiCl)(y) changes the superconducting properties of the grains as well as of the intergrain matrix. The splitting of the peak in the temperature dependence of the imaginary part of the complex susceptibility, corresponding to the dissipation inside the grains, was also observed.

AC complex susceptibility (with and without a superimposed DC field) and DC magnetization measurements on (Bi,Pb)-2223 high-temperature superconductors with various amounts of LiF are presented. The results are discussed in the frame of the critical state model. The values of the intra- and inter-granular critical current density as well as of fields for full penetration are estimated. It can be seen that, in Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiF)(y), various amounts of LiF change the superconducting properties of both the grains and the inter-grain matrix. The intra-granular critical current density has similar values from both AC susceptibility and DC magnetization measurements, its highest value being attained for y = 0.15. For all LiF-doped samples, a split of the peak corresponding to the dissipation in the grains was observed. (C) 2002 Elsevier Science B.V. All rights reserved.

From ac susceptibility measurements of the [Bi(Pb)](2)Ca2Sr2Cu3Oz (Bi-2223) samples doped with LiCl, we have found and report for the first time anomalously suppressed superconductivity (T, is anomalously decreasing) in the slightly under-doped region. For our BPSCCO/(LiCl)(y) samples this region is situated around y = 0.07. Hole concentration (p) per number of Cu-O planes of the Bi-2223 unit cell, determined from room temperature thermopower (S-300 K) measurements, is approximately 0.15 when y is within anomalous region. Literature data shows that for the La-based cuprates, similar suppression of superconductivity was observed at p similar to 0.12 (so-called "1/8 problem"). This discrepancy would appear because charge ordering phenomenon (probably induced by Li known as a pair breaker as e.g. Zn) may be accompanied by changes in oxygen content or oxygen ordering effects. (C) 2003 Elsevier B.V. All rights reserved.

We studied the YBa2Cu3O7-x bulk superconductor doped with BaZrO3 up to 50 wt.%, obtained by solid-state reaction powder technology. From DC magnetization loops and low frequency AC susceptibility measurements we determined the influence of the BaZrO3 doping level on the critical temperature, critical current density, field for full penetration, and intergrain lower critical field. The results show that even high content of BaZrO3 does not lead to degradation of the superconducting properties of bulk YBa2Cu3O7-x.

We investigated the superconducting critical temperature, transport critical-current density and the thermo-power properties of Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox/(LiF)(y) samples. It was found that the midpoint critical temperature increases with increasing y, attaining approximate to 119.5 K for y = 0.15. The transition width shows a minimum and the critical temperature (zero electrical resistance) exhibits a maximum as a function of y. The observed behavior is correlated with the SEM analysis. Powder X-ray diffraction studies reveal that in our samples the amount of Bi2Sr2Ca2Cu3O10+delta high-temperature superconducting phase is maximal (70-78%) for y = 0.05-0.07.

Thin films of YBa2Cu3O7-x have been obtained on NdGaO3 substrate by pulsed laser deposition with an excimer KrF* (lambda =248 nm, tau (FWHM)greater than or equal to 20 ns) laser source from a stoichiometric target. In the present paper we report details of the technology of pulsed laser deposition of high-temperature superconductor thin films, substrates' requirements and high-temperature superconductor thin film characterisation. The study of some parameters' intercorelations for optimisation of the technology of the pulsed laser deposition of high-temperature superconductor thin films is also analysed Moreover, the contacting technology and techniques of characterisation are described.

DC magnetization and AC complex susceptibility measurements on (Bi,Pb) : 2223 high-temperature superconductors impurified with various amounts of BaZrO3 are presented. The results are discussed in the frame of the critical state model. and the values of the inter- and intragranular critical current density as well as of the field for full penetration are estimated. The values of the intergranular critical current density are consistent with those obtained from transport measurements. The intragranular critical current density and the field for full penetration have similar values from both DC magnetization and AC susceptibility measurements. It was shown that, in the (Bi,Pb) : 2223 system. BaZrO3 impurification changes only the properties of the intergrain matrix, while the superconducting properties of the grains are not modified.